HRID24544

反应详情

EQUATION

反应方程式

HRID 24544 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 5-formyl-4-(2-ethoxycarbonylethyl)-3-methyl-1H-pyrrole-2-carboxylic acid ethyl ester (281 mg), 5-bromo-2-oxindole (220 mg), and piperidine (2 drops) in ethanol (2 mL) was stirred at 90° C. for 2 hours. Potassium hydroxide (537 mg) was added and the temperature was increased to 95° C. for 1 hour. The reaction mixture was cooled and concentrated. The residue was dissolved into water and acidified with 2 N hydrochloric acid to pH 2. The precipitate that formed was filtered, washed with water and dried in a vacuum oven overnight to give 411 mg (98%) of 4-(2-carboxyethyl)-3-methyl-5-(5-bromo-2-oxo-1,2-dihydro-indol-3-ylidenemethyl)-1H-pyrrole-2-carboxylic acid.

WORKUP

后处理

  1. temperaturethe temperature was increased to 95° C. for 1 hour
  2. temperatureThe reaction mixture was cooled
  3. concentrationconcentrated
  4. dissolutionThe residue was dissolved into water
  5. customThe precipitate that formed
  6. filtrationwas filtered
  7. washwashed with water
  8. customdried in a vacuum oven overnight